Methanesulfonic Acid → 4-(3,6-dihydro-2H-pyran-4-yl)benzonitrile
反応式
CS(O)(=O)=O.O[C:7]1([C:13]2[CH:20]=[CH:19][C:16]([C:17]#[N:18])=[CH:15][CH:14]=2)[CH2:12][CH2:11][O:10][CH2:9][CH2:8]1.[BH4-].[Na+].[OH-].[Na+]>C(Cl)Cl>[O:10]1[CH2:9][CH:8]=[C:7]([C:13]2[CH:20]=[CH:19][C:16]([C:17]#[N:18])=[CH:15][CH:14]=2)[CH2:12][CH2:11]1参加物
6
実験手順
12.65 ml (195 mmol) MeSO3H in 10 ml CH2Cl2 was slowly added to a mixture of 611 mg (3.0 mmol) 4-(4-hydroxytetrahydro-2H-pyran-4-yl)benzonitrile and 1.13 g (30 mmol) NaBH4 in 15 ml CH2Cl2 at 0° C. Stirred for 1 h. 2M NaOH was added until pH>10. The mixture was extracted with CH2Cl2. The organic phase was dried (MgSO4) and concentrated. The crude product (450 mg, 81%) was used directly in the next step.
後処理
- extractionThe mixture was extracted with CH2Cl2
- dry with materialThe organic phase was dried (MgSO4)
- concentrationconcentrated
出典と根拠
- ORDレコード
- ord-71a78143f7674dfc95cc65c37a91402f
- 出典データセット
- uspto-grants-2013_04
- 特許番号
- US08415333B2
反応ノート
読み込み中…